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CN119592097B - Preparation method of red organic pigment for liquid crystal color filter material - Google Patents

Preparation method of red organic pigment for liquid crystal color filter material

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Publication number
CN119592097B
CN119592097B CN202411786441.9A CN202411786441A CN119592097B CN 119592097 B CN119592097 B CN 119592097B CN 202411786441 A CN202411786441 A CN 202411786441A CN 119592097 B CN119592097 B CN 119592097B
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slurry
liquid crystal
color filter
pigment
organic pigment
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CN119592097A (en
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高小良
李国文
丁红桂
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Cairui New Materials Jiangsu Co ltd
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Cairui New Materials Jiangsu Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B48/00Quinacridones
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0002Grinding; Milling with solid grinding or milling assistants
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0084Dispersions of dyes
    • C09B67/0085Non common dispersing agents
    • C09B67/009Non common dispersing agents polymeric dispersing agent
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K19/00Liquid crystal materials
    • C09K19/52Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
    • C09K19/60Pleochroic dyes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Optical Filters (AREA)

Abstract

The invention discloses a preparation method of a red organic pigment for a liquid crystal color filter material, which comprises the following steps of adding a hyperbranched polymer nano dispersing agent into ethyl acetate, adding a pigment red 122 crude product and calcium chloride to obtain mixed slurry, adding the mixed slurry into a ball mill to grind to obtain ground slurry, transferring the ground slurry into a dodecylamine polyoxyethylene ether aqueous solution, stirring and preserving heat, filtering to obtain surface modified slurry, adding the surface modified slurry into a DMF (dimethyl formamide) solution containing the hyperbranched polymer nano dispersing agent, carrying out ultrasonic treatment, filtering to obtain final slurry, and drying to obtain the red organic pigment. By improving the pigment processing technology, pigment particles are thinned to the nanometer level, and the dispersion stability and the fluidity of the pigment are improved. The prepared red organic pigment has uniform particle size distribution, high color purity and good optical performance, and is suitable for a color filter of a liquid crystal display.

Description

Preparation method of red organic pigment for liquid crystal color filter material
Technical Field
The invention relates to the technical field of pigments, in particular to a preparation method of a red organic pigment for a liquid crystal color filter material.
Background
Color Liquid Crystal Displays (LCDs) are one of the most common display devices today, and are widely used in various electronic products such as televisions, computers, mobile phones, and the like. The display principle of the liquid crystal display is mainly to realize the Color display of images by matching a Color Filter (CF) with a liquid crystal material. The color filter is generally composed of red, green and blue sub-pixels, and each sub-pixel forms a corresponding color by backlight provided by a light source. Specifically, the backlight controls light transmission through each pixel unit of the color filter by switching on and off the liquid crystal in each of the three sub-pixels of red, green, and blue, thereby generating a complete color image.
The red, green and blue colors in the color filter are mainly transmitted through different organic pigment layers to realize light transmission with specific wavelength and provide required color expression. Organic pigments have high color saturation and good light resistance, and thus are widely used in displays. In color filters, the use of pigments is generally required to have high color purity, good transparency, and to maintain stable color under long-term illumination. Common red organic pigments include quinacridones (Quinacr idone), diketopyrrolopyrroles (Diketopyrrolopyrrole, DPP) and the like, and the pigments have high color vividness and excellent light resistance and are an important material source of color filters.
In the coating process of the color filter, the organic pigment is required to be attached to the filter substrate with extremely high dispersion uniformity to ensure uniformity of the color development effect thereof. The dispersibility of pigment particles directly affects the transparency and durability of the filter. In the conventional preparation process, the pigment is usually required to achieve nanocrystallization by means of superfine grinding, ultrasonic dispersion and the like, but these methods still have limitations in terms of uniformity of pigment particle distribution, accuracy of size control and stability of dispersion. In addition, the organic pigment has poor storage stability in a dispersion medium, and tends to easily aggregate or settle, resulting in formation of an uneven colored layer during the coating process of the filter.
Disclosure of Invention
Based on the problems existing in the background technology, the invention provides a preparation method of a red organic pigment for a liquid crystal color filter material, pigment particles are thinned to a nanometer level by improving the processing technology of the pigment, and the dispersion stability and the fluidity of the pigment are improved by specific dispersion treatment. The prepared red organic pigment has uniform particle size distribution, high color purity and good optical performance, and is suitable for a color filter of a liquid crystal display.
The invention is implemented by the following technical scheme:
A method for preparing a red organic pigment for a liquid crystal color filter material, comprising the following steps:
S1, adding a hyperbranched polymer nano dispersing agent into ethyl acetate, continuously adding a pigment red 122 crude product and calcium chloride, and uniformly mixing to obtain mixed slurry;
s2, adding the mixed slurry into a ball mill, and carrying out wet grinding to obtain ground slurry;
s3, transferring the ground slurry into a dodecylamine polyoxyethylene ether aqueous solution, stirring, preserving heat, and filtering to obtain a surface modified slurry;
S4, adding the surface modified slurry into DMF solution containing hyperbranched polymer nano-dispersants, performing ultrasonic treatment, and filtering to obtain final slurry;
s5, drying the final slurry to obtain the red organic pigment for the liquid crystal color filter material.
Further, the hyperbranched polymer nano-dispersant in the step S1 is a hyperbranched polyacrylamide-methyl acrylate copolymer.
The preparation method of the hyperbranched polyacrylamide-methyl acrylate copolymer comprises the steps of adding acrylamide and methyl methacrylate into DMF solution, adding ethylene glycol dimethacrylate, stirring uniformly, heating to 60 ℃ under the protection of nitrogen, sequentially adding azodiisobutyronitrile to initiate polymerization reaction, stirring for 8-10h, slowly dripping the reaction solution into glacial ethanol after the reaction is finished for precipitation, washing and drying to obtain the hyperbranched polyacrylamide-methyl acrylate copolymer.
Further, the mass ratio of the acrylamide to the methyl methacrylate is 1 (2-5), the dosage of the ethylene glycol dimethacrylate is 4-6% of the total mass of the acrylamide, and the dosage of the azodiisobutyronitrile is 0.1-1% of the total mass of the acrylamide and the methyl methacrylate.
Further, in the step S1, the raw material components comprise, by weight, 2-5 parts of hyperbranched polymer nano-dispersants, 80-120 parts of pigment red 122 crude products, 100-200 parts of calcium chloride and 25-40 parts of ethyl acetate.
Further, in the step S2, zirconia beads with the diameter of 0.5-1mm are adopted as grinding media in the wet grinding, the rotating speed of the ball mill is 800-1000 revolutions per minute, the grinding time is 10-12 hours, and the grinding temperature is lower than 40 ℃.
Further, in the step S3, the mass fraction of the dodecylamine polyoxyethylene ether aqueous solution is 2-3%, the heat preservation temperature is 50-60 ℃ and the time is 3-4h.
Further, in the step S3, the mass ratio of the ground slurry to the aqueous solution of the dodecylamine polyoxyethylene ether is 1 (1-2).
Further, in the step S4, the mass fraction of the hyperbranched polymer nano-dispersant in the DMF solution containing the hyperbranched polymer nano-dispersant is 2-3%, and the ultrasonic treatment is carried out for 30-60min.
Further, the mass ratio of the surface modified slurry to the DMF solution containing the hyperbranched polymer nano-dispersant in the step S4 is 1 (1.5-3).
The invention has the beneficial effects that:
1. The dispersant used in the invention is a hyperbranched polymer, and the hyperbranched polymer has a highly branched structure, so that the dispersant can be effectively dispersed in a liquid phase. This helps to improve the dispersion state of the pigment in the solution, prevent aggregation or precipitation of the pigment, and thereby improve the stability and uniformity of the pigment. In particular in liquid crystal display applications, uniform dispersion of pigments is critical to achieving high quality color.
2. The dodecylamine polyoxyethylene ether is added to the surface of the pigment through surface modification, so that the compatibility of the pigment and the liquid crystal material is improved. This is important to ensure uniformity and stability of the liquid crystal color filter material, and particularly in a liquid crystal display, good compatibility of the pigment with the substrate effectively improves the display effect. In addition, the surface modification is helpful for the functionalization of the pigment, and improves the optical performance, chemical resistance, heat resistance and the like.
3. And hyperbranched polymer nano-dispersants are added into the slurry after surface modification, so that the dispersion stability of the pigment is further enhanced. The two-stage dispersant application can ensure the long-term stability of pigment in the liquid crystal color filter material and avoid the reagglomeration of pigment particles. The hyperbranched polymer is used as the dispersing agent, so that the optical effect of the pigment can be effectively improved, the color purity is improved, the light scattering and shielding effects among particles are reduced, and the brightness and the color contrast of the liquid crystal color filter material are further enhanced.
4. The red organic pigment prepared by the method has the advantages of finer granularity and good dispersion, and after the surface modification, the compatibility with the liquid crystal display screen substrate can be improved, the optical performance of the red organic pigment is further improved, and the color accuracy and the color vividness are ensured. In liquid crystal color filter applications, the red organic pigment is effective in regulating light transmittance and light reflection, providing more stable and accurate color. The use of surface modified and hyperbranched polymers gives pigments with greater chemical and light resistance, especially in the context of liquid crystal displays, where the pigments need to withstand a variety of chemical media and ultraviolet light irradiation. The pigment can keep its color stable and prolong its service life.
Detailed Description
The technical scheme of the present invention will be further described in detail with reference to the following specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
A method for preparing a red organic pigment for a liquid crystal color filter material, comprising the following steps:
S1, preparing a hyperbranched polymer nano dispersing agent, namely adding 10 parts of acrylamide and 30 parts of methyl methacrylate into DMF (dimethyl formamide) solution, adding 1 part of ethylene glycol dimethacrylate, uniformly stirring, heating to 60 ℃ under the protection of nitrogen, sequentially adding 0.33 part of azobisisobutyronitrile to initiate polymerization reaction, stirring for 8-10 hours, slowly dripping the reaction solution into glacial ethanol after the reaction is finished, precipitating and washing, and drying to obtain the hyperbranched polyacrylamide-methyl acrylate copolymer;
s2, adding 3 parts of hyperbranched polymer nano-dispersing agent into 25 parts of ethyl acetate, continuously adding 100 parts of pigment red 122 crude product and 150 parts of calcium chloride, and uniformly mixing to obtain mixed slurry;
S3, adding the mixed slurry into a ball mill, adopting zirconia beads with the diameter of 0.5-1mm as a grinding medium, wherein the rotating speed of the ball mill is 800 revolutions per minute, the grinding time is 12 hours, the grinding temperature is lower than 40 ℃, and wet grinding is carried out to obtain ground slurry;
S4, transferring the ground slurry into a dodecylamine polyoxyethylene ether aqueous solution with the mass fraction of 2%, stirring and preserving heat for 3 hours at 60 ℃ with the mass ratio of the ground slurry to the dodecylamine polyoxyethylene ether aqueous solution being 1:1, and filtering to obtain surface modified slurry;
S5, adding the surface modified slurry into a DMF solution containing 2% of hyperbranched polymer nano-dispersing agent by mass, wherein the mass ratio of the surface modified slurry to the DMF solution containing the hyperbranched polymer nano-dispersing agent is 1:2, carrying out ultrasonic treatment for 30min, and filtering to obtain the final slurry;
s6, drying the final slurry to obtain the red organic pigment for the liquid crystal color filter material.
Example 2
The difference between this example and example 1 is that in step S2, 5 parts of hyperbranched polymer nano-dispersant is added into 25 parts of ethyl acetate, 90 parts of crude pigment red 122 and 150 parts of calcium chloride are continuously added and uniformly mixed to obtain a mixed slurry, and the rest steps are the same as in example 1.
Comparative example 1
The dispersant used was WI NSPERSE 3200 (new vitamin materials, inc.);
The preparation method comprises the following specific steps:
S1, adding 3 parts of dispersing agent WI NSPERSE 3200 into 25 parts of ethyl acetate, continuously adding 100 parts of pigment red 122 crude product and 150 parts of calcium chloride, and uniformly mixing to obtain mixed slurry;
s2, adding the mixed slurry into a ball mill, adopting zirconia beads with the diameter of 0.5-1mm as a grinding medium, wherein the rotating speed of the ball mill is 800 revolutions per minute, the grinding time is 12 hours, the grinding temperature is lower than 40 ℃, and wet grinding is carried out to obtain ground slurry;
S3, transferring the ground slurry into a dodecylamine polyoxyethylene ether aqueous solution with the mass fraction of 2%, stirring and preserving heat for 3 hours at 60 ℃ with the mass ratio of the ground slurry to the dodecylamine polyoxyethylene ether aqueous solution being 1:1, and filtering to obtain surface modified slurry;
s4, drying the final slurry to obtain the red organic pigment for the liquid crystal color filter material.
Comparative example 2
The comparative example is different from example 1 in that the dispersant used is polyacrylamide-methyl acrylate copolymer, which is prepared by adding 30 parts of acrylamide and 10 parts of methyl methacrylate into 50 parts of DMF solution, adding 1 part of ethylene glycol dimethacrylate, stirring uniformly, heating to 60 ℃ under the protection of nitrogen, sequentially adding 0.33 part of azobisisobutyronitrile to initiate polymerization reaction, stirring for 8-10 hours, cooling to room temperature, slowly dripping the reaction solution into glacial ethanol to precipitate after the reaction is finished, washing, and drying, thus obtaining the polyacrylamide-methyl acrylate copolymer, and the rest steps are the same as those of example 1.
Comparative example 3
The comparative example is different from example 1 in that the preparation step does not include step S5, the modified slurry prepared in step S4 is directly freeze-dried, and the rest steps are the same as example 1.
Application example 1
The pigment of example 1 was prepared as a red paste, and the specific method was that 5.7g of a red organic pigment, 4.5g of a grinding resin BM52 (Shanghai Borile chemical industry production), 2.3g of a grinding aid WI NSPERSE3030 (Uygur-Site New Material (Weibos New Material Co., ltd.), 25.5g of propylene glycol methyl ether acetate, and 0.1mm of zirconium balls were added to a grinding tank, and mixed and dispersed for 24 hours by a Miq double planetary dynamic ball mill to obtain a red paste.
Application example 2
The pigment obtained in example 2 was used in the same amount as that of the pigment of example 1 used in application example 1, and the other components and the amounts of the components and the operation process were the same as those of application example 1.
Comparative application example 1
The pigment obtained in comparative example 1 was used in place of the pigment of example 1 used in application example 1 in an equivalent weight, and the remaining components and the amounts of the components and the operation process were the same as those in application example 1.
Comparative application example 2
The pigment of comparative example 2 was used in place of the pigment of example 1 used in application example 1 in an equivalent weight, and the remaining components and amounts of the components and the operation process were the same as those of application example 1.
Comparative application example 3
The pigment of comparative example 3 was used in place of the pigment of example 1 used in application example 1 in an equivalent weight, and the remaining components and amounts of the components and the operation process were the same as those of application example 1.
Comparative application example 4
The pigment of example 1 employed in application example 1 was replaced with an equivalent weight of untreated commercially available pigment Red 122, and the remaining components and amounts of components and the operation process were the same as those of application example 1.
The performance test was performed on the red paste prepared in application examples 1-2 and comparative application examples 1-3.
Particle size testing
The average particle diameter and the particle diameter distribution of the red paste obtained in the application example and comparative application example were measured by using a particle size analyzer 90 pl us.
Viscosity test and dispersion stability test
The red paste prepared in application examples 1-2 and comparative application examples 1-3 was left to stand at room temperature for 1 day, sampled, and the initial viscosity was measured using a viscometer DV2T, and the remaining red paste was left to stand at 40℃for 7 days, sampled, and the viscosity was measured using a viscometer DV2T for 7 days.
Chemical resistance
The red paste obtained in the application example and the comparative application example was put into a 230 ℃ oven for 30 minutes by spin-coating a coating film on a 6cm×6cm glass sheet, pre-baking at 120 ℃ for 3 minutes.
The prepared smear was immersed in Propylene Glycol Monomethyl Ether Acetate (PGMEA) solvent at 60 ℃ for 10 minutes, and the color change before and after evaluation was observed. Here, the color change was calculated using the following equation, and the value calculated using the equation is shown in table 1 below.
ΔEab*=[(ΔL*)2+(Δa*)2+(Δb*)2]1/2
Δl, Δa, Δb in the equation represent the color change defined by L, a, and b observed using a three-dimensional colorimeter.
Evaluation criteria
Good chemical resistance (no pattern change, delta (Eab) less than 3.0)
Delta chemical resistance generally (slight pattern change, delta (Eab. X) of 3.0 to less than 5.0)
Poor chemical resistance (pattern change, delta (Eab) of 5.0 or more)
Smear contrast test
The smear was measured by a contrast tester (japanese pot motor CT-1) for the ratio of the brightness of the polarizing plate in the orthogonal position to the brightness of the polarizing plate in the parallel position, i.e., the contrast. Assuming that the contrast obtained by the test of comparative application example 4 is 100, the contrast values obtained by the test of other application examples and comparative application examples are compared with each other to obtain the contrast data shown in table 1.
All test results are shown in table 1.
TABLE 1
As can be seen from the data in Table 1, the red color paste prepared in the examples 1 and 2 of the invention has smaller average particle size, narrower particle size distribution and better storage stability, and the prepared smear has good chemical resistance and has obvious advantages as compared with the commercial pigment red 122. The red organic pigment prepared by the invention can be used for preparing a colorant of a red pixel point of a liquid crystal color filter material. The dispersant WI NSPERSE 3200 is adopted in the preparation of the comparative example 1, and the dodecylamine polyoxyethylene ether aqueous solution is directly filtered and dried after being treated in the preparation process, and the dispersant is not adopted for secondary treatment, so that the performances of the finally obtained red color paste are reduced. In the preparation of comparative example 2, the polyacrylamide-methyl acrylate copolymer is used as a dispersing agent, the dosage of polyacrylamide and methyl methacrylate is adjusted, the finally prepared copolymer is more biased to a linear structure rather than hyperbranched, and the improvement of the dosage of acrylamide leads to the enhancement of the hydrophilicity of the copolymer, which is not beneficial to the improvement of the dispersibility of the organic pigment, so that the performance of the final color paste is also reduced. In comparative example 3, after wet grinding, the mixture is treated by an aqueous solution of dodecylamine polyoxyethylene ether, and then the mixture is directly filtered and dried, and a dispersant is not used for secondary treatment, so that the dispersion stability of the red color paste is reduced, and the color contrast is slightly reduced.
In one embodiment, the method for preparing the red organic pigment for the liquid crystal color filter material, after the red organic pigment for the liquid crystal color filter material, further comprises:
S6, detecting the standard of the obtained red organic pigment for the liquid crystal color filter material, when the detection condition parameter reflects that the standard detection is unqualified, adaptively making a preparation flow problem tracing model based on the detection condition parameter, tracing the problems of the preparation flow (at least comprising the steps S1 to S5), and solving the tracing acquisition problem on line;
in S6, the adaptively formulating a traceability model of the preparation process problem based on the detection condition parameters includes:
s611, extracting characteristics of the detection condition parameters to obtain a plurality of parameter characteristics;
In S611, the detection condition parameters are various result parameters for detecting the standard of the obtained red organic pigment for the liquid crystal color filter material, standard indexes are preset, and the detection condition parameters are generated based on the difference relation between the detection result and the standard indexes;
s612, mapping each parameter characteristic with a problem map to obtain a plurality of mapping problems, wherein the mapping problems are problems corresponding to root nodes and branch nodes of a tree-shaped data structure of all leaf nodes occupied by each parameter characteristic in the problem map;
In S612, the problem map has a plurality of tree-shaped data structures, in a tree-shaped data result, a root node is the beginning of a detection flow problem, the root node diverges to have a plurality of branch edges, the branch edges have a plurality of branch nodes, one branch edge represents the change process of a problem parameter of the detection flow problem, the branch nodes connected in sequence are a plurality of process items of the change process, the terminal of one branch edge is a leaf node, and the leaf node is the change result of a problem parameter;
S613, generating templates based on the problem tracing rules, and generating a plurality of problem tracing rules according to each mapping problem;
in S613, the problem tracing rule is a rule that whether a mapping problem exists in the tracing preparation flow;
S614, formulating a preparation flow problem tracing model based on each problem tracing rule;
In S614, finally, a preparation flow problem tracing model is formulated based on each problem tracing rule, and during preparation, a plurality of problem tracing rules can be ordered regularly to form a system work module for sequentially executing the rules, which is used as the preparation flow problem tracing model;
in S6, the online solving the tracing obtaining problem includes:
S621, carrying out knowledge demand analysis on the traceability acquisition problem to acquire a plurality of knowledge demands;
in S621, when the knowledge demand analysis is performed, what knowledge needs to be acquired to solve the traceability acquisition problem, i.e. the knowledge demand is analyzed;
s622, traversing all knowledge requirements in sequence;
S623, analyzing the requirement types of the traversed knowledge requirements each time, wherein the requirement types are divided into active requirements and passive requirements;
In S623, the demand types of the knowledge demands are divided into two types, active and passive, wherein active refers to that the knowledge demands can be based on acquired knowledge alone;
S624, when the requirement type of the knowledge requirement is an active requirement, acquiring corresponding first target knowledge based on the knowledge requirement;
In S624, the first target knowledge may be in the form of expert experience or the like;
S625, combining knowledge requirements with the requirement type being a passive requirement to obtain a combined knowledge requirement, and acquiring corresponding second target knowledge based on the combined knowledge requirement;
in S625, the second target knowledge may be in the form of expert experience, etc., and may meet all knowledge requirements for joining;
s626, generating a problem solving strategy based on the first target knowledge and the second target knowledge;
in S626, after the first target knowledge and the second target knowledge are acquired, a problem-solving policy is generated based on both;
s627, solving the traceability acquisition problem on line based on the problem solving strategy.
In S627, finally, the problem obtained by tracing is solved on line based on the problem solving strategy, wherein on line means that the system carries out corresponding adjustment control on equipment control related to the preparation flow.
The embodiment of the invention has the following beneficial effects:
1. In the prior art, many manufacturing processes often rely on empirical or fixed detection criteria to identify and solve problems. However, in the embodiment, the problem traceability model is introduced through self-adaptive feedback of the standard detection result in the preparation process, so that accurate analysis can be performed aiming at specific reasons of each detection failure. Compared with the traditional preparation flow, when quality failure occurs, the method can perform deep analysis through an automatic problem traceability model, so that problems in preparation are fundamentally searched, and the preparation quality is improved.
2. The problem diagnosis in the prior art is often solved by manual detection and manual analysis, and has low efficiency and easily ignores potential factors. According to the embodiment, through detection parameter feature extraction, a detection result is converted into quantifiable feature data, and then the feature data and a problem map are mapped to obtain a plurality of potential problems, so that comprehensive and efficient problem tracing is realized. The tree structure of the problem map helps to realize multi-level and multi-angle analysis, can more comprehensively identify and analyze the root cause of the problem, and avoids missing important factors.
3. In the process of tracing the problem, the embodiment determines the required knowledge type through knowledge demand analysis, and obtains expert experience or other relevant knowledge according to the demand type. The differentiation of the active requirement and the passive requirement enables the learning and obtaining process to be more accurate and efficient, and can effectively support on-line adjustment and problem solving.
4. By introducing the self-adaptive problem tracing model, knowledge demand analysis, expert experience combination and on-line control adjustment, the automation level, the intelligent level and the problem solving efficiency of the preparation process of the red organic pigment for the liquid crystal color filter material are remarkably improved, and the problems can be rapidly positioned and solved when the problems occur, so that quality fluctuation and resource waste in production are reduced.
Finally, it should be noted that the above-mentioned embodiments only represent several embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the concept of the present invention should be included in the scope of the present invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (7)

1.一种用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,包括以下步骤:1. A method for preparing a red organic pigment for liquid crystal color filter material, characterized in that it comprises the following steps: S1.将超支化聚合物纳米分散剂加入到乙酸乙酯中,继续加入颜料红122粗品和氯化钙,混合均匀,得到混合浆料;S1. The hyperbranched polymer nanodispersant was added to ethyl acetate, and crude Pigment Red 122 and calcium chloride were added, mixed uniformly to obtain a mixed slurry; S2.将混合浆料加入到球磨机中,湿法研磨,得到研磨后浆料;S2. The mixed slurry is added to a ball mill and wet-ground to obtain a ground slurry; S3.将研磨后浆料转移至十二烷基胺聚氧乙烯醚水溶液中,搅拌保温,过滤,得到表面改性浆料;S3. The ground slurry was transferred to an aqueous solution of polyoxyethylene dodecylamine ether, stirred and heated, and filtered to obtain a surface-modified slurry; S4.将表面改性浆料加入到包含超支化聚合物纳米分散剂的DMF溶液中,超声波处理,过滤,得到最终浆料;S4. adding the surface modified slurry to a DMF solution containing a hyperbranched polymer nanodispersant, ultrasonically treating, and filtering to obtain a final slurry; S5.将最终浆料进行干燥,即得用于液晶滤色材料的红色有机颜料;S5. The final slurry is dried to obtain a red organic pigment for a liquid crystal color filter material; 步骤S1中超支化聚合物纳米分散剂为超支化聚丙烯酰胺-丙烯酸甲酯共聚物;In step S1, the hyperbranched polymer nanodispersant is a hyperbranched polyacrylamide-methyl acrylate copolymer; 超支化聚丙烯酰胺-丙烯酸甲酯共聚物的制备方法具体为:将丙烯酰胺和甲基丙烯酸甲酯加入到DMF溶液中,加入乙二醇二甲基丙烯酸酯,搅拌均匀;在氮气保护下,加热至60℃,依次加入偶氮二异丁腈引发聚合反应,搅拌反应8-10h后,反应结束后将反应液缓慢滴入冰乙醇中进行沉淀,洗涤,过滤,干燥,即得超支化聚丙烯酰胺-丙烯酸甲酯共聚物;The preparation method of the hyperbranched polyacrylamide-methyl acrylate copolymer is specifically as follows: acrylamide and methyl methacrylate are added to a DMF solution, ethylene glycol dimethacrylate is added, and the mixture is stirred evenly; under nitrogen protection, the mixture is heated to 60° C., azobisisobutyronitrile is added in sequence to initiate a polymerization reaction, the reaction mixture is stirred for 8-10 hours, and after the reaction is completed, the reaction solution is slowly dripped into ice ethanol for precipitation, washed, filtered, and dried to obtain the hyperbranched polyacrylamide-methyl acrylate copolymer; 丙烯酰胺和甲基丙烯酸甲酯的质量比为1:(2-5);乙二醇二甲基丙烯酸酯的用量占丙烯酰胺总质量的4-6%;偶氮二异丁腈用量占丙烯酰胺和甲基丙烯酸甲酯总质量的0.1-1%。The mass ratio of acrylamide to methyl methacrylate is 1:(2-5); the amount of ethylene glycol dimethacrylate accounts for 4-6% of the total mass of acrylamide; and the amount of azobisisobutyronitrile accounts for 0.1-1% of the total mass of acrylamide and methyl methacrylate. 2.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S1中各原料组分按重量份计具体为:超支化聚合物纳米分散剂2-5份、颜料红122粗品80-120份、氯化钙100-200份、乙酸乙酯25-40份。2. The method for preparing a red organic pigment for liquid crystal color filter materials according to claim 1, characterized in that the raw material components in step S1 are specifically: 2-5 parts of hyperbranched polymer nanodispersant, 80-120 parts of crude Pigment Red 122, 100-200 parts of calcium chloride, and 25-40 parts of ethyl acetate in parts by weight. 3.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S2中湿法研磨采用直径为0.5-1mm的氧化锆珠作为研磨介质,球磨机的转速为800-1000转/min,研磨时间为10-12h,研磨温度低于40℃。3. The method for preparing a red organic pigment for liquid crystal color filter materials according to claim 1 is characterized in that in step S2, zirconium oxide beads with a diameter of 0.5-1 mm are used as grinding media for wet grinding, the speed of the ball mill is 800-1000 rpm, the grinding time is 10-12 h, and the grinding temperature is lower than 40°C. 4.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S3中十二烷基胺聚氧乙烯醚水溶液的质量分数为2-3%;保温温度为50-60℃,时间为3-4h。4. The method for preparing a red organic pigment for liquid crystal color filter material according to claim 1, characterized in that the mass fraction of the dodecylamine polyoxyethylene ether aqueous solution in step S3 is 2-3%; the insulation temperature is 50-60°C and the time is 3-4h. 5.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S3中研磨后浆料与十二烷基胺聚氧乙烯醚水溶液的质量比为1:(1-2)。5. The method for preparing a red organic pigment for a liquid crystal color filter material according to claim 1, characterized in that the mass ratio of the slurry after grinding to the aqueous solution of dodecylamine polyoxyethylene ether in step S3 is 1:(1-2). 6.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S4中包含超支化聚合物纳米分散剂的DMF溶液中超支化聚合物纳米分散剂的质量分数为2-3%,超声波处理30-60min。6. The method for preparing a red organic pigment for liquid crystal color filter material according to claim 1, characterized in that the mass fraction of the hyperbranched polymer nanodispersant in the DMF solution containing the hyperbranched polymer nanodispersant in step S4 is 2-3%, and the ultrasonic treatment is carried out for 30-60 min. 7.根据权利要求1所述的用于液晶滤色材料的红色有机颜料的制备方法,其特征在于,步骤S4中表面改性浆料和包含超支化聚合物纳米分散剂的DMF溶液的质量比为1:(1.5-3)。7. The method for preparing a red organic pigment for a liquid crystal color filter material according to claim 1, characterized in that the mass ratio of the surface modified slurry to the DMF solution containing the hyperbranched polymer nanodispersant in step S4 is 1:(1.5-3).
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CN101117450A (en) * 2007-07-23 2008-02-06 江南大学 A kind of preparation method of nonionic hyperbranched polymer dispersant for organic pigment
CN104212239A (en) * 2014-09-04 2014-12-17 江南大学 Method for improving color fastness of pigment ink by using multifunctional hyperbranched dispersant

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101117450A (en) * 2007-07-23 2008-02-06 江南大学 A kind of preparation method of nonionic hyperbranched polymer dispersant for organic pigment
CN104212239A (en) * 2014-09-04 2014-12-17 江南大学 Method for improving color fastness of pigment ink by using multifunctional hyperbranched dispersant

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